Abstract: Instructed by H-bonding specific sequencing, a new method was designed to synthesize block copolymer β-CD-PLA with disulfide bond linkages. The structure of block copolymer β-CD-PLA was characterized by ¹H-NMR and GPC, and pyrene was used as fluorescence probe to characterize properties of copolymers of β-CD-PLA self-assembled micelles. The Dynamic Light Scattering (DLS) nano-particle size analyzer was used to characterize the size of the self-assembled micelles. As a result, the intermediates remove the protecting group to form the target block copolymer β-CD-PLA with disulfide bonds instructed by H-bonding and the oxidation of I₂, and the critical micelle concentration (CMC) value is 0.089 mg/mL, which suggests the micelle is highly stable in dilute solution. The particle size of blank micelles is 31 nm, and the particle size of the loaded micelles is 42 nm, which is self-assembled by block copolymer β-CD-PLA.